Thermal insulation — Test methods for specific heat capacity of thermal insulation for buildings in the high temperature range — Differential scanning calorimetry (DSC) method

This document specifies test methods for specific heat capacity under high temperature conditions from the normal temperature range to 1 600 K for insulation materials for buildings using the differential scanning calorimetry (DSC) method.

Isolation thermique — Méthodes d'essai relatives à la capacité thermique massique de l'isolation thermique des bâtiments dans la plage de température élevée — Méthode par calorimétrie à balayage différentiel (DSC)

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Status
Published
Publication Date
09-Jan-2023
Current Stage
6060 - International Standard published
Due Date
12-Jun-2022
Completion Date
10-Jan-2023
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ISO 24144:2023 - Thermal insulation — Test methods for specific heat capacity of thermal insulation for buildings in the high temperature range — Differential scanning calorimetry (DSC) method Released:10. 01. 2023
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INTERNATIONAL ISO
STANDARD 24144
First edition
2023-01
Thermal insulation — Test methods
for specific heat capacity of thermal
insulation for buildings in the high
temperature range — Differential
scanning calorimetry (DSC) method
Isolation thermique — Méthodes d'essai relatives à la capacité
thermique massique de l'isolation thermique des bâtiments dans la
plage de température élevée — Méthode par calorimétrie à balayage
différentiel (DSC)
Reference number
ISO 24144:2023(E)
© ISO 2023
---------------------- Page: 1 ----------------------
ISO 24144:2023(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2023

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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Published in Switzerland
© ISO 2023 – All rights reserved
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ISO 24144:2023(E)
Contents Page

Foreword ..........................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 1

4 Principles ..................................................................................................................................................................................................................... 2

4.1 General ........................................................................................................................................................................................................... 2

4.2 Heat-flux DSC ........................................................................................................................................................................................... 2

4.3 Power-compensation DSC ............................................................................................................................................................. 3

5 Method ............................................................................................................................................................................................................................ 4

5.1 General ........................................................................................................................................................................................................... 4

5.2 Basic procedure ..................................................................................................................................................................................... 5

6 Apparatus and materials ............................................................................................................................................................................7

6.1 DSC apparatus ......................................................................................................................................................................................... 7

6.2 Crucibles ....................................................................................................................................................................................................... 8

6.2.1 General ........................................................................................................................................................................................ 8

6.2.2 Shape, material and mass ........................................................................................................................................... 8

6.2.3 Measurement temperature range ....................................................................................................................... 8

7 Test specimen .......................................................................................................................................................................................................... 8

7.1 General ........................................................................................................................................................................................................... 8

7.2 Sampling ....................................................................................................................................................................................................... 9

7.3 Moulding ...................................................................................................................................................................................................... 9

8 Test conditions and specimen conditioning ........................................................................................................................... 9

8.1 Test conditions ........................................................................................................................................................................................ 9

8.2 Conditioning of specimens ........................................................................................................................................................... 9

9 Calibration ..................................................................................................................................................................................................................9

9.1 General ........................................................................................................................................................................................................... 9

9.2 Calibration materials ..................................................................................................................................................................... 10

10 Procedure .................................................................................................................................................................................................................10

10.1 Setting up the apparatus ............................................................................................................................................................ 10

10.2 Loading the specimen into the crucible ........................................................................................................................ 10

10.2.1 General ..................................................................................................................................................................................... 10

10.2.2 Selection of crucibles ................................................................................................................................................... 10

10.2.3 Weighing the specimen crucible........................................................................................................................ 10

10.2.4 Loading the specimen ................................................................................................................................................. 10

10.2.5 Determination of the mass of the specimen ........................................................................................... 11

10.3 Performing measurements ....................................................................................................................................................... 11

10.4 Post-run checks ................................................................................................................................................................................... 11

11 Determination of specific heat capacities ..............................................................................................................................11

11.1 General ........................................................................................................................................................................................................ 11

11.2 Calculation of specific heat capacities ............................................................................................................................ 11

11.2.1 In case of near-match with isothermal baselines of DSC curves .......................................... 11

11.2.2 In case of discordance with isothermal baseline of DSC curves ...........................................12

11.3 Numerical rounding of the results .....................................................................................................................................12

12 Test report ...............................................................................................................................................................................................................12

Annex A (normative) DSC apparatus for high temperature range ...................................................................................14

Annex B (normative) Moulding procedure of test specimen ..................................................................................................15

Annex C (informative) Analysis method considering discordance of isothermal baseline ...................18

Annex D (informative) Materials for DSC calibrations ..................................................................................................................20

iii
© ISO 2023 – All rights reserved
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ISO 24144:2023(E)

Bibliography .............................................................................................................................................................................................................................21

© ISO 2023 – All rights reserved
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ISO 24144:2023(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

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electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

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www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 163, Thermal performance and energy use

in the built environment, Subcommittee SC 1, Test and measurement methods.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www.iso.org/members.html.
© ISO 2023 – All rights reserved
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INTERNATIONAL STANDARD ISO 24144:2023(E)
Thermal insulation — Test methods for specific heat
capacity of thermal insulation for buildings in the high
temperature range — Differential scanning calorimetry
(DSC) method
1 Scope

This document specifies test methods for specific heat capacity under high temperature conditions from

the normal temperature range to 1 600 K for insulation materials for buildings using the differential

scanning calorimetry (DSC) method.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 11357-1:20—, Plastics — Differential scanning calorimetry (DSC) — Part 1: General principles

ISO 11357-4:2021, Plastics — Differential scanning calorimetry (DSC) — Part 4: Determination of specific

heat capacity
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 11357-1, ISO 11357-4 and the

following apply.

ISO and IEC maintain terminology databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
specific heat capacity

quantity of heat necessary to raise the temperature of a unit mass of material by 1 K at constant

pressure
Note 1 to entry: It is given by the following formula:
1dQ
 
c =× (1)
 
m dT 
where
−1 −1

c is the specific heat capacity and is expressed in kilojoules per kilogram per K (kJ⋅kg ⋅K )

−1 −1

or in joules per gram per K (J⋅g ⋅K ); subscript p indicates an isobaric process;

m is the mass of material, expressed in kilogram (kg) or gram (g);
1) Under preparation. Stage at time of publication: ISO/FDIS 11357-1.
© ISO 2023 – All rights reserved
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ISO 24144:2023(E)

dQ is the quantity of heat dQ necessary to raise the temperature of the material by dT, expressed

 
 
−1 −1

in kilojoules per K (kJ⋅K ) or in joules per K (J⋅K ), measured at constant pressure.

 
3.2
specimen

item which is cut from thermal insulation material and processed into powder form or compression

moulded for measurement by differential scanning calorimetry (DSC)
Note 1 to entry: See Annex B for further information on moulding procedure.
3.3
reference material
material of known specific heat capacity (3.1)
Note 1 to entry: See ISO 11357-4:2021, Annex A for further information.
3.4
calibration material
material of known temperature and heat of fusion
Note 1 to entry: See Annex D for further information on calibration materials.
3.5
three-step temperature control method

method that consists of isothermal maintenance at the start temperature, constant heating step at the

middle temperature and isothermal maintenance at the end temperature
3.6
differential scanning calorimetry
DSC

method in which the difference in energy inputs into a substance and a reference material is measured

as a function of temperature while the substance and reference material are subjected to a controlled

temperature programme
[SOURCE: ISO/TS 80004-6:2021, 6.2.1]
4 Principles
4.1 General

DSC is a method in which the difference in energy inputs into a substance and a reference material is

measured as a function of temperature while the substance and reference material are subjected to a

controlled temperature programme.

The difference between the rate of heat flow into a specimen and the rate of heat flow into a reference

crucible is measured as a function of either temperature or time, or both, while the specimen and the

reference are subjected to the same temperature-control programme under a specified atmosphere.

The measurements can be undertaken using two types of DSC: heat-flux DSC and power-compensation

DSC.
4.2 Heat-flux DSC

The specimen and reference positions are subjected to the same temperature-control programme by a

single heater. A difference in temperature, ΔT, occurs between the specimen position and the reference

position because of the difference in heat capacity between the specimen and the reference. From

this temperature difference, the difference in the rates of heat flow into the specimen and reference

positions is derived and is normally recorded against the temperature of the reference, T , or against

ref
time.
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ISO 24144:2023(E)
A schematic drawing of a heat-flux DSC instrument is shown in Figure 1.
Key
1 sample holder 6 heating furnace
2 reference holder T temperature at sample holder (T )
1 specimen
3 crucible T temperature at reference holder (T )
2 ref
4 stage ΔT temperature difference between sample and reference holder
5 thermopile
Figure 1 — Schematic diagram illustrating the basic principles of heat-flux DSC
4.3 Power-compensation DSC

In power-compensated DSC, individual heaters are used for the specimen and reference positions.

The difference in electrical power required to maintain both the specimen position and the reference

position at the same temperature is recorded against temperature or time, while each position is

subjected to the same temperature-control programme.

For power-compensated isoperibolic calorimeters, the surrounding temperature (i.e. the temperature

of the heat sink) shall be kept constant.
A schematic drawing of a power-compensation DSC instrument is shown in Figure 2.
© ISO 2023 – All rights reserved
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ISO 24144:2023(E)
Key
1 specimen position 6 heat-flux compensation circuit
2 reference position 7 surrounding heat sink
3 thermometers T temperature at specimen position (T )
1 specimen
4 individual heaters T temperature at reference position (T )
2 ref
5 measurement circuit for T and
specimen
ref

Figure 2 — Schematic diagram illustrating the basic principles of power-compensation DSC

5 Method
5.1 General

This document specifies methods for the measurement of specific heat capacity according to the heat-

flux DSC method and the power-compensation DSC method, based on the three-step temperature

control method.

The apparatus for both methods comprises two measuring cells (sample holders) housed in a furnace

which provides overall system heating. One cell contains the test specimen within a crucible, and the

other contains an empty crucible only.
a) Power-compensation DSC method

Each cell has an individual heater to compensate for temperature variations from the overall heating

programme. The power which is supplied to either cell heater to maintain equal temperatures

during heating is measured.
b) Heat-flux DSC method

Power is exchanged between each cell and its respective surrounding during the heating

programme. The difference in power exchange between the two cells is measured.
© ISO 2023 – All rights reserved
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